CN106086561B - The preparation method of gradient graphene/magnesium base composite material - Google Patents
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Abstract
Organic monomer hydroxyethyl methacrylate, crosslinking agent trimethylolpropane trimethacrylate, dispersant oleic acid, magnesium powder and Graphene powder, are distributed in n-butanol are prepared into graphene/magnesium complex phase slurry first by a kind of preparation method of gradient graphene/magnesium base composite material；Initiator benzoyl peroxide and catalyst n, N dimethyl aniline are added after ball milling in slurry；It will be centrifuged in the graphene configured/magnesium slurry injection centrifuge, graphene and magnesium granules in slurry is formed continuous gradient distribution；Mould is placed on into PhastGel in vacuum drying oven after centrifugation to solidify；Sample after gel solidification is placed in argon gas atmosphere in tube furnace and sinters gradient graphene/magnesium bio-medical composition into after the demoulding, vacuum drying.So as to improve the decay resistance and mechanical property of magnesium matrix.
Description
Technical field
The present invention is a kind of preparation method of gradient graphene/magnesium base composite material.
Background technology
Magnesium alloy is used as biomedical metallic material and other biomedical metallic material phases through clinical usage now
Than having a clear superiority：（1）Aboundresources, cheap, reserves of the magnesium in the earth's crust are extremely enriched, and its reserves reaches
2.8%, occupy the 6th；（2）Magnesium is one of indispensable mineral matter element of human body, and magnesium almost participates in human body all new old generations
Apologize for having done sth. wrong journey, its content is only second to potassium, magnesium influence potassium, sodium, " passage " of the movement of calcium ion intraor extracellular in the cell, and has dimension
Hold the effect of biological film potential；（3）Good mechanical compatibility, the modulus of elasticity and density using magnesium as the alloy of matrix is closest
Skeleton modulus of elasticity and density；（4）Excellent biocompatibility and biodegradable, magnesium alloy in itself can in organism
Gradually to degrade, original implant is gradually replaced by freshman bone tissue, is preferable biologic bracket material.But magnesium metal
It is active high, it is more serious by corrosion in body fluid phenomenon in vivo.Mismatched within (12~18 weeks) with new bone growth speed, so carrying
Its high corrosion resistance, it is magnesium and alloy as bone renovating material it still is able to keep mechanical performance before new bone growth is intact
Need most the key issue of solution.Graphene has good biocompatibility and chemical stability, no cytotoxicity, graphene
And its derivative uses broadness in terms of Nano medication transportation system, biological inspection, bio-imaging, tumour are cured.With stone
Black alkene can be used in bacterium anatomy, DNA and protein inspection etc. for the biological plant or biology sensor of bottom.But how will
Graphene adds less with the decay resistance and mechanical property research that improve magnesium matrix in magnesium matrix.
The content of the invention
It is an object of the invention to solve it is the problems of above-mentioned there is provided it is a kind of improve magnesium matrix decay resistance and
The preparation method of gradient graphene/magnesium base composite material of mechanical property.
The technical scheme is that：
First by organic monomer hydroxyethyl methacrylate（HEMA）, crosslinking agent trimethylolpropane trimethacrylate
（TMPTA）, dispersant oleic acid, magnesium powder and Graphene powder be distributed in n-butanol and be prepared into graphene/magnesium complex phase slurry；After ball milling
Initiator benzoyl peroxide is added in slurry（BPO）And catalyst n, N dimethyl aniline（DMA）；It will configure afterwards
Centrifuged in graphene/magnesium slurry injection centrifuge, graphene and magnesium granules in slurry is formed continuous gradient distribution；Centrifugation
Mould is placed on into PhastGel in vacuum drying oven afterwards to solidify；Sample after gel solidification is placed in after the demoulding, vacuum drying
Argon gas atmosphere sinters gradient graphene/magnesium bio-medical composition into tube furnace.
1st, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 5-15 parts of organic monomer hydroxyethyl methacrylates（HEMA), 1-3 parts of crosslinking agent trihydroxy methyls
Propane triacrylate（TMPTA）In the n-butanol for being dissolved into 29.125-60.25 parts, stir, 1.5- is added afterwards
2.25 parts of dispersant oleic acid, stir, and are subsequently added magnesium powder and 3-4.5 parts of granularity 500nm that 27-40.5 parts of granularities are 60nm
Graphene powder, stir；2-5 parts of initiator benzoyl peroxides are added after ball milling 24h（BPO）With 0.25-0.625 parts
Catalyst n, N dimethyl aniline（DMA）, stir, be prepared into graphene/magnesium complex phase slurry.
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium complex phase slurry prepared is injected into centrifuge in mould, in 500-2000r/min
10-20min is centrifuged under rotating speed, graphene and magnesium granules is formed continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 60-80 DEG C of vacuum drying oven, after the green compact demoulding after solidification
3-6h is dried in 100-150 DEG C of vacuum drying oven, be then placed in tube furnace under argon gas atmosphere protection sinter into gradient graphene/
Magnesium base composite material.Its sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3
DEG C/min heating rate is as cold as room temperature after being heated to 610-630 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.4-0.8
L/min。
The advantage of the invention is that：
1. propose a kind of novel preparation method of gradient graphene/magnesium base composite material, gradient-structure schematic diagram such as Fig. 1 institutes
Show.In the sample prepared by the technique graphene particles form the distribution of continuous gradient in magnesium matrix, it is to avoid conventional dry
The defect such as layering and crackle present in molded sample, can be by graphene film in magnesium matrix after graphene while adding
Carrying and extraction, the bridge joint of crackle and deflecting effect improve the mechanical property of magnesium-based composite material.（As shown in table 1）.
The mechanical property of gradient graphene/magnesium base composite material prepared by the different process of table 1（Graphene content is 10 wt%）
2. in gradient graphene/magnesium base composite material, the higher one end of graphene content has good biocompatibility
And corrosion resistance（As shown in table 2）, while graphene can be with Ca in induction body fluid2+And PO4 3-Ion deposition, on magnesium matrix surface
Hydroxyapatite layer is generated, accelerates the growth of new bone, and then the healing of bone tissue and the degraded of magnesium alloy is matched, reduction is planted
Enter unsuccessfully the generation of phenomenon.And there is the high one end of magnesium matrix content higher intensity and toughness preferably to be held in implantation process
Carry on a shoulder pole extraneous load.
The corrosion rate of the pure magnesium of table 2 and gradient graphene/magnesium base composite material（Graphene content is 20 wt%）
Brief description of the drawings
Fig. 1 is gradient graphene/magnesium schematic diagram.
Embodiment
With reference to embodiment, the present invention will be further described：
Example 1
1st, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 5 parts of organic monomer hydroxyethyl methacrylates（HEMA), 1 part of crosslinking agent trimethylolpropane
Triacrylate（TMPTA）In the n-butanol for being dissolved into 60.25 parts, stir, 1.5 parts of dispersant oleic acid added afterwards,
Stir, it is 60nm magnesium powder and 3 parts of granularity 500nm Graphene powder to be subsequently added 27 parts of granularities, is stirred；Ball milling
2 parts of initiator benzoyl peroxides are added after 24h（BPO）With 0.25 part of catalyst n, N dimethyl aniline（DMA）, stirring is
It is even, graphene/magnesium complex phase slurry is made.
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium complex phase slurry prepared is injected into centrifuge in mould, in 500r/min rotating speeds
Lower centrifugation 20min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 60 DEG C of vacuum drying ovens, after the demoulding of green compact after solidification
6h is dried in 100 DEG C of vacuum drying ovens, is then placed in tube furnace and sinters gradient graphene/magnesium composite wood under argon gas atmosphere protection
Material；Its sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min liter
Warm speed is as cold as room temperature after being heated to 610 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.4L/min.
Example 2
1st, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 15 parts of organic monomer hydroxyethyl methacrylates（HEMA), 3 parts of crosslinking agent trimethylolpropanes
Triacrylate（TMPTA）In the n-butanol for being dissolved into 29.125 parts, stir, 2.25 parts of dispersant oil are added afterwards
Acid, stirs, and it is 60nm magnesium powder and 4.5 parts of granularity 500nm Graphene powder to be subsequently added 40.5 parts of granularities, and stirring is equal
It is even；5 parts of initiator benzoyl peroxides are added after ball milling 24h（BPO）With 0.625 part of catalyst n, N dimethyl aniline
（DMA）, stir, graphene/magnesium complex phase slurry be made.
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, under 2000r/min rotating speeds from
Heart 10min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 80 DEG C of vacuum drying ovens, after the demoulding of green compact after solidification
3h is dried in 150 DEG C of vacuum drying ovens, is then placed in tube furnace and sinters gradient graphene/magnesium composite wood under argon gas atmosphere protection
Material；Its sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min liter
Warm speed is as cold as room temperature after being heated to 630 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.8 L/min.
Example 3
1st, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 10 parts of organic monomer hydroxyethyl methacrylates（HEMA), 2 parts of crosslinking agent trimethylolpropanes
Triacrylate（TMPTA）In the n-butanol for being dissolved into 47.875 parts, stir, 1.75 parts of dispersant oil are added afterwards
Acid, stirs, and it is 60nm magnesium powder and 3.5 parts of granularity 500nm Graphene powder to be subsequently added 31.5 parts of granularities, and stirring is equal
It is even；3 parts of initiator benzoyl peroxides are added after ball milling 24h（BPO）With 0.375 part of catalyst n, N dimethyl aniline
（DMA）, stir, graphene/magnesium complex phase slurry be made.
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, under 1000r/min rotating speeds from
Heart 15min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 70 DEG C of vacuum drying ovens, after the demoulding of green compact after solidification
4h is dried in 120 DEG C of vacuum drying ovens, is then placed in tube furnace and sinters gradient graphene/magnesium composite wood under argon gas atmosphere protection
Material；Its sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min liter
Warm speed is as cold as room temperature after being heated to 620 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.5 L/min.
Example 4
1st, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 10 parts of organic monomer hydroxyethyl methacrylates（HEMA), 2 parts of crosslinking agent trimethylolpropanes
Triacrylate（TMPTA）In the n-butanol for being dissolved into 41.5 parts, stir, 2 parts of dispersant oleic acid are added afterwards, stir
Uniformly, it is 60nm magnesium powder and 4 parts of granularity 500nm Graphene powder to be subsequently added 36 parts of granularities, is stirred；After ball milling 24h
Add 4 parts of initiator benzoyl peroxides（BPO）With 0.5 part of catalyst n, N dimethyl aniline（DMA）, stir, stone be made
Black alkene/magnesium complex phase slurry.
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, under 1500r/min rotating speeds from
Heart 15min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 75 DEG C of vacuum drying ovens, after the demoulding of green compact after solidification
5h is dried in 130 DEG C of vacuum drying ovens, is then placed in tube furnace and sinters gradient graphene/magnesium composite wood under argon gas atmosphere protection
Material；Its sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min liter
Warm speed is as cold as room temperature after being heated to 620 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.6L/min.
Claims (5)
1. a kind of preparation method of gradient graphene/magnesium base composite material, it is characterised in that
First, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 5-15 parts of organic monomer hydroxyethyl methacrylates, 1-3 parts of crosslinking agent trimethylolpropane tris propylene
Acid esters is dissolved into 29.125-60.25 parts of n-butanol, is stirred, and 1.5-2.25 parts of dispersant oleic acid are added afterwards, are stirred
Mix uniform, it is 60nm magnesium powder and 3-4.5 parts of granularity 500nm Graphene powder to be subsequently added 27-40.5 parts of granularities, stirring is equal
It is even；2-5 parts of initiator benzoyl peroxides and 0.25-0.625 parts of catalyst n, N dimethyl aniline are added after ball milling 24h, is stirred
Mix uniform, be prepared into graphene/magnesium complex phase slurry；
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium complex phase slurry prepared is injected into centrifuge in mould, in 500-2000r/min rotating speeds
Lower centrifugation 10-20min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 60-80 DEG C of vacuum drying oven, after the demoulding of green compact after solidification
3-6h is dried in 100-150 DEG C of vacuum drying oven, is then placed in tube furnace and sinters gradient graphene/magnesium under argon gas atmosphere protection
Composite；Its sintering process is：Be heated to 300 DEG C from room temperature using 1 DEG C/min heating rate, after insulation 3h, with 3 DEG C/
Min heating rate is as cold as room temperature after being heated to 610-630 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.4-0.8 L/
min。
2. a kind of preparation method of gradient graphene/magnesium base composite material according to described in claim 1, it is characterised in that
First, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 5 parts of organic monomer hydroxyethyl methacrylates, 1 part of crosslinking agent trimethylolpropane trimethacrylate
In the n-butanol for being dissolved into 60.25 parts, stir, add 1.5 dispersant oleic acid, stir, be subsequently added 27 parts of grains
The Graphene powder for 60nm magnesium powder and 3 parts of granularity 500nm is spent, is stirred；2 parts of initiator peroxidating are added after ball milling 24h
Benzoyl and 0.25 part of catalyst n, N dimethyl aniline stir, and graphene/magnesium complex phase slurry is made；
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium complex phase slurry prepared is injected into centrifuge in mould, under 500r/min rotating speeds from
Heart 20min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 60 DEG C of vacuum drying ovens, at 100 DEG C after the green compact demoulding after solidification
6h is dried in vacuum drying oven, is then placed in tube furnace and sinters gradient graphene/magnesium base composite material under argon gas atmosphere protection；Its
Sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min heating speed
Rate is as cold as room temperature after being heated to 610 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.4L/min.
3. a kind of preparation method of gradient graphene/magnesium base composite material according to described in claim 1, it is characterised in that
First, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 15 parts of organic monomer hydroxyethyl methacrylates, 3 parts of crosslinking agent trimethylolpropane trimethacrylates
In the n-butanol for being dissolved into 29.125 parts, stir, add 2.25 parts of dispersant oleic acid, stir, be subsequently added
40.5 parts of granularities are 60nm magnesium powder and 4.5 parts of granularity 500nm Graphene powder, are stirred；5 parts are added after ball milling 24h to draw
Agent benzoyl peroxide and 0.625 part of catalyst n, N dimethyl aniline are sent out, is stirred, graphene/magnesium complex phase slurry is made
Material；
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, centrifuged under 2000r/min rotating speeds
10min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 80 DEG C of vacuum drying ovens, at 150 DEG C after the green compact demoulding after solidification
3h is dried in vacuum drying oven, is then placed in tube furnace and sinters gradient graphene/magnesium base composite material under argon gas atmosphere protection；Its
Sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min heating speed
Rate is as cold as room temperature after being heated to 630 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.8 L/min.
4. a kind of preparation method of gradient graphene/magnesium base composite material according to described in claim 1, it is characterised in that
First, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 10 parts of organic monomer hydroxyethyl methacrylates, 2 parts of crosslinking agent trimethylolpropane trimethacrylates
In the n-butanol for being dissolved into 47.875 parts, stir, 1.75 parts of dispersant oleic acid are added afterwards, are stirred, then add
It is 60nm magnesium powder and 3.5 parts of granularity 500nm Graphene powder to enter 31.5 parts of granularities, is stirred；3 parts are added after ball milling 24h
Initiator benzoyl peroxide and 0.375 part of catalyst n, N dimethyl aniline stir, and graphene/magnesium complex phase slurry is made
Material；
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, centrifuged under 1000r/min rotating speeds
15min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 70 DEG C of vacuum drying ovens, at 120 DEG C after the green compact demoulding after solidification
4h is dried in vacuum drying oven, is then placed in tube furnace and sinters gradient graphene/magnesium base composite material under argon gas atmosphere protection；Its
Sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min heating speed
Rate is as cold as room temperature after being heated to 620 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.5 L/min.
5. a kind of preparation method of gradient graphene/magnesium base composite material according to described in claim 1, it is characterised in that
First, the preparation of graphene/magnesium complex phase slurry
By mass fraction, by 10 parts of organic monomer hydroxyethyl methacrylates, 2 parts of crosslinking agent trimethylolpropane trimethacrylates
In the n-butanol for being dissolved into 41.5 parts, stir, add 2 parts of dispersant oleic acid, stir, be subsequently added 36 parts of granularities
The Graphene powder of magnesium powder and 4 parts of granularity 500nm for 60nm, stirs；4 parts of initiator benzoyl peroxides are added after ball milling 24h
Formyl and 0.5 part of catalyst n, N dimethyl aniline, stir, and graphene/magnesium complex phase slurry is made；
2nd, centrifugation, gel solidification and sintering
A. the above-mentioned graphene/magnesium slurry prepared is injected into centrifuge in mould, centrifuged under 1500r/min rotating speeds
15min, makes graphene and magnesium granules form continuous gradient distribution；
B. the slurry after centrifugation is put into gel solidification 30min in 75 DEG C of vacuum drying ovens, at 130 DEG C after the green compact demoulding after solidification
5h is dried in vacuum drying oven, is then placed in tube furnace and sinters gradient graphene/magnesium base composite material under argon gas atmosphere protection；Its
Sintering process is：It is heated to using 1 DEG C/min heating rate from room temperature after 300 DEG C, insulation 3h, with 3 DEG C/min heating speed
Rate is as cold as room temperature after being heated to 620 DEG C, insulation 2h with stove；Wherein the flow velocity of argon gas is 0.6L/min.
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| CN105112694A (en) * | 2015-06-25 | 2015-12-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method of magnesium base graphene alloy |
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